CN115463070B

CN115463070B - Hybrid flower extract and preparation method thereof

Info

Publication number: CN115463070B
Application number: CN202210745375.5A
Authority: CN
Inventors: 蔡彬弟; 林柳城
Original assignee: Guangdong Fanmilin Biotechnology Co ltd
Current assignee: Guangdong Fanmilin Biotechnology Co ltd
Priority date: 2022-06-27
Filing date: 2022-06-27
Publication date: 2023-08-22
Anticipated expiration: 2042-06-27
Also published as: CN115463070A

Abstract

The application relates to the field of daily cosmetics, A61K8/00, in particular to a hybrid flower extract. The application discloses a hybrid flower extract, which comprises the following raw materials in parts by weight: mixing vegetable oil, polymer containing hydroxyl and ether bond, and hybridization flower, wherein the hybridization flower can be one of black rose, china rose, camellia, pomegranate flower and lily. The application utilizes various chemical environments and unique structures constructed by mixing vegetable oil and polymer containing hydroxyl and ether bond, extracts more antioxidant active substances from the hybrid flower through various intermolecular action modes, and ensures that the extract exists more stably in the constructed system.

Description

Hybrid flower extract and preparation method thereof

Technical Field

The application relates to the field of daily cosmetics, A61K8/00, in particular to a hybrid flower extract.

Background

The skin can undergo oxidation reaction after long-term irradiation of sunlight and computer and exposure to polluted air and color cosmetics, and generates free radicals which have strong oxidability, damage organism tissues and cells and cause aging. The oxidation of the free radical to the skin is carried out at all times, and the oxidized skin has the main symptoms of dark complexion, uneven complexion, dry skin, fine lines, spots and the like, which affect the beauty and health of the skin, and the addition of the antioxidant can solve or alleviate the skin problems in daily skin care and cosmetics.

Antioxidants fall into two categories: one is a water-soluble polar antioxidant (e.g., vitamin C); the other is a fat-soluble nonpolar antioxidant (such as vitamin E); in cosmetic emulsions (aqueous phase + oil phase), it is very useful to add these two types of antioxidants to protect the skin. In the oil-water mixed phase, the nonpolar antioxidants will diffuse in the oil to protect it from dissolved oxygen; for polar or moderately polar antioxidants (e.g. phenols, vitamin C) will aggregate and disperse at the air/oil or water/oil interface, whereas in this interface polar or moderately polar substances are very easily oxidized.

CN108785192a discloses a mineral oil-free natural cosmetic skin care product with natural components and no toxic or side effect and a preparation method thereof, wherein the adopted vegetable oil phase is isononyl isononanoate, cetyl isonicotinate, almond oil, sunflower oil, linseed oil, blackcurrant oil, grape seed oil, kiwi fruit oil, wheat germ oil, jin Guisuan glyceride, wheat germ emulsifying wax, sodium polyacrylate polymer, glyceryl monostearate, cetostearyl alcohol and butter fruit; the oil-water co-dissolution is obtained in the balanced emulsification process, and according to the selection of components, series of skin care products with different effects can be obtained, so that the skin problems of pore blocking, sensitization, acne, black spots and the like are solved. CN106983708A discloses a propolis whitening skin care product and a preparation method thereof, wherein the propolis is prepared from various flavonoid compounds, various alkene, terpenoid compounds, trace amino acids, vitamin B groups, mineral substances, trace elements, various organic acids and the like, the skin antioxidation, moisturizing and anti-aging capabilities of the propolis are improved, the skin elasticity is increased, the skin immunity is enhanced, and the freckle, chloasma, butterfly spot and the like of the face of a human body are removed.

However, none of these techniques take into account the stability of these antioxidant substances in the resulting system, except for the content of the effective antioxidant components in the extract. Because the raw materials in the cosmetic system are complex, the formula often contains grease and other easily oxidized components, a perfect antioxidant system needs to be established in the formula to prevent the product from deteriorating due to oxidization, and meanwhile, the stability of the antioxidant system needs to be improved to prevent the antioxidant system from losing efficacy.

Disclosure of Invention

In order to solve the technical problems, the application provides a hybrid flower extract, which comprises the following raw materials: mixing vegetable oil, polymer containing hydroxyl and ether bond, and hybrid flower, wherein the hybrid flower is one of black rose (rosa nigra), rose (rosa flower), camellia (camellia), pomegranate flower (flos mali granati) and lily (lilium).

The hybrid flower is used as plant resource, contains a large amount of polyphenols (including flavonoids) active substances, such as gallic acid, quercetin, catechin, rutin, multivitamins and the like, and has strong antioxidation capability on oxidative free radicals; the effective antioxidant substances are extracted and applied to skin care or cosmetics, and can be used for moisturizing, keeping moisture, keeping skin tender and luster, removing wrinkles and black spots, and delaying skin aging.

Oil is a very complex system containing more or less polar fat-soluble components; structural and biological functional similarities exist between fatty acids in vegetable oils, phytosterols … … and lipids in skin; the application selects different vegetable oil combinations, utilizes the synergistic effect among the mixed vegetable oils to extract more antioxidant substances in the hybrid flowers and ensures that the antioxidant substances exist stably in the system.

The mixed vegetable Oil is a combination of several of shea butter (shea butter), seabuckthorn seed Oil (Mare Buckhorn semen Oleum), cactus seed Oil (Semen Oleum Cactus), avocado Oil (Avocado Oil), juicy peach kernel Oil (Persici Oleum Kernel), almond Oil (Oleum amygdalinum), sunflower Oil (Helianthus Oleum), macadamia Oil (Macadamia Oil), linseed Oil (Oil line), jojoba Oil (Jojoba Oil), coconut Oil (Cocoes Oil), kiwi seed Oil (Kiwi seed Oil) and blackcurrant Oil (blackcurrant Oleum).

Preferably, the raw materials comprise, by weight: 3-11% of polymer containing hydroxyl and ether bond, 9-25% of hybrid flower and the balance of mixed vegetable oil to 100%.

Further, in order to make the extract of the hybrid flowers contain more antioxidant active substances and simultaneously ensure the stability and extraction rate of the antioxidant active substances, we limit the weight ratio of the hybrid flowers to the mixed vegetable oil to be 10:1-1:10.

in some preferred embodiments, the blend of vegetable oils is selected from jojoba oil (CAS# 61789-91-1) and blackcurrant oil (CAS# 68606-81-5), which better enhances the antioxidant capacity and stability of the extract, because: the jojoba oil and blackcurrant oil molecules contain a large number of unsaturated bonds, carboxyl groups, hydroxyl groups and unique molecular structures, and the chemical bonds interact in different ways and also are combined with various antioxidant molecules in the hybrid flowers in different ways, so that more antioxidant molecules are extracted and stably exist.

Further, in some preferred embodiments, the weight ratio of jojoba oil to blackcurrant oil is 8:1-1:8. preferably, the weight ratio of the jojoba oil to the blackcurrant oil is 5:1-1:5.

the types and the amounts of unsaturated bonds, carboxyl groups and hydroxyl groups contained in the molecules of the jojoba oil and the blackcurrant oil are different, and the molecular structures of the jojoba oil and the blackcurrant oil are also greatly different in space; the relative amounts of the polar bonds and the nonpolar bonds contained in the mixed vegetable oil are controlled by limiting the weight ratio of the polar bonds and the nonpolar bonds, and the spatial structure of the mixed vegetable oil is influenced, so that the extraction process of the hybrid flowers is influenced.

The polymer containing hydroxyl and ether bond, wherein the number of the hydroxyl is more than or equal to 3, and the number of the ether bond is more than 2; the molecular chain of the polymer and the polar functional group contained in the polymer are combined with antioxidant molecules in the extract in different modes, so that the intermolecular binding force is enhanced, and the number of antioxidant active substances in the hybrid flower extract is increased.

Further preferred is one of polyglyceryl-4 oleate (CAS# 71012-10-7), polyglyceryl-3 diisostearate (CAS# 63705-03-3), polysorbate-60 (CAS: 9005-67-8); in a preferred embodiment, the polyglycerin-4 oleate is present in an amount of 3% to 11% by weight of the total hybrid flower extract.

The polyglycerol-4 oleate is a long-chain substance containing hydroxyl, ether bond and unsaturated chemical bond, wherein the functional groups are combined with polar and nonpolar components in jojoba oil and blackcurrant oil in different modes to create different polar/nonpolar, semi-polar/semi-nonpolar, polar/semi-nonpolar and other environments, more polar and nonpolar antioxidant substances in the hybrid flower are extracted through the synergistic effect of the three, and the antioxidant substances in the extract are not easy to be oxidized and lose efficacy after being stored for a long time in a system constructed by the three.

Furthermore, the dosage of the polyglycerol-4 oleate is limited, the synergistic effect between the polyglycerol-4 oleate and the mixed vegetable oil is regulated, the component environment of the system is better coordinated, and the antioxidant substance content in the hybrid flower extract is further improved by combining with antioxidant active molecules in the hybrid flower in various intermolecular action modes, so that the hybrid flower extract is not easy to be oxidized and lose efficacy.

The preparation method of the hybrid flower extract comprises the following steps:

(1) Drying the hybridized flower;

(2) Grinding the hybridized flower treated in the step (1) at a low temperature;

(3) Uniformly mixing the hybridized flower powder obtained by grinding in the step (2), mixed vegetable oil and a polymer containing hydroxyl and ether bonds, and then carrying out microwave (power: 2450MHz-6 kW) and ultrasonic (10 kHz-80 kHz) treatment;

(4) And (3) carrying out coarse filtration on the substance obtained in the step (3), and then carrying out centrifugal separation to obtain the hybridized flower extract.

The temperature of the low-temperature grinding is-60 to-100 ℃, and the grinding is carried out for 40-60 minutes.

In the step (3): microwave and ultrasonic wave alternate extraction for 4-6 times, each time for 1-10 minutes.

In a preferred embodiment, the flowers in step (1) are reserved with a moisture content of 5% to 20%.

Advantageous effects

More antioxidant active substances in the hybrid flowers are extracted by utilizing the synergistic effect, molecular structure and various chemical environments constructed by the mixed vegetable oil and the polymer containing hydroxyl and ether bonds, and the antioxidant active substances exist in the system stably; the hybrid flower extract prepared by the technical scheme has very high total polyphenol content, capability of scavenging free radicals and excellent stability.

Detailed Description

Examples

Example 1:

a hybrid flower extract is prepared from the following raw materials: 3% of polymer containing hydroxyl and ether bond, 9% of hybrid flower and 88% of mixed vegetable oil.

Wherein: the polymer containing hydroxyl and ether bond is polyglycerol-4 oleate; the mixed vegetable oil is jojoba oil and blackcurrant oil, and the weight ratio of the jojoba oil to the blackcurrant oil is 5:1.

the preparation method comprises the following steps:

(1) And drying the black rose in a low-temperature constant-temperature control room, wherein 10% of water is reserved.

(2) Grinding the black rose treated in the step (1) at a low temperature of-80 ℃ for 50 minutes.

(3) Uniformly mixing the black rose powder, the jojoba oil, the blackcurrant oil and the polymer containing hydroxyl and ether bonds, which are obtained by grinding in the step (2), and then adding the mixture into dynamic cold-temperature extraction equipment, and carrying out alternating extraction by microwaves (power 6 kW) and ultrasonic treatment (80 kHz) for 5 times, wherein the time length of each extraction is 5 minutes;

(4) Coarse filtering the substance obtained in the step (3) by using a flat filter, and then performing centrifugal separation to obtain the hybridized flower extract.

Example 2:

the difference from example 1 is that: the raw materials comprise: 11% of polymer containing hydroxyl and ether bond, 25% of hybrid flower and 64% of mixed vegetable oil; the weight ratio of the jojoba oil to the blackcurrant oil is 1:5, the preparation and other parameters were in accordance with example 1.

Example 3:

the difference from example 1 is that: the polymer containing hydroxyl and ether bond is polyglycerol-3 diisostearate; the preparation process and other parameters were in accordance with example 1.

Example 4:

the difference from example 1 is that: the raw materials comprise: 0% of polymer containing hydroxyl and ether bond, 28% of hybrid flower and 72% of mixed vegetable oil; the addition amount of the polymer containing hydroxyl and ether bond in the step (3) of the preparation method is 0; the preparation process and other parameters were in accordance with example 1.

Example 5:

the difference from example 1 is that the weight ratio of jojoba oil to blackcurrant oil is 1:0. raw material information:

1. jojoba oil: CAS#61789-91-1;

2. blackcurrant oil: CAS#68606-81-5;

3. polyglycerol-3 diisostearate: CAS#63705-03-3;

4. polyglycerol-4 oleate: CAS#71012-10-7;

5. the black rose is Bacarat black rose.

Performance test method

1. Measurement of peroxide value:

peroxide value of the extract at the time of production (meqO) ₂ Evaluation criteria of/kg): the peroxide value is preferably less than 1.5; the peroxide value of 1.5 is less than or equal to 3; the peroxide value is equal to or higher than 3.

Change in peroxide number after 15 days at 40℃in a BeqO ₂ Evaluation criteria of/kg): the absolute value of the change quantity of the peroxide value is preferably less than 0.5; the absolute value of the change quantity of the peroxide value which is more than or equal to 0.5 and less than 1 is recorded as a middle value; the absolute value of the change amount of the peroxide value of 1.ltoreq.peroxide is recorded as a difference.

Example test results are shown in table 1.

2. Total polyphenol content test

The Folin-Ciocalteu method is used: mixing 0.5mL of the hybrid flower extract and 0.5mL of Folin-Ciocalteu reagent at 0.25mol/L, standing for 3 min, and adding 1mL of 15% Na ₂ CO ₃ And after standing for 30 minutes, centrifuging for 3 minutes using a high-speed centrifugal disperser (3500 r/min); with 15% Na ₂ CO ₃ The solution served as a blank and the absorbance of the centrifuged supernatant was measured at 760 nm. Preparing a series of phenol solutions with standard concentration, measuring the absorbance according to the same measuring method, establishing a standard curve of the phenol concentration and the corresponding absorbance, and substituting the absorbance value of the sample into the curve to obtain the phenol concentration of the sample. The measurement results of the 3 samples are shown in Table 1, and the results are averaged over two parallel experiments. Example test results are shown in table 1.

Evaluation criteria for total polyphenol content (mg/kg equivalent Oleuropein): the total polyphenol content is more than or equal to 10000 and is recorded as excellent; the total polyphenol content of 4000 is less than 10000; total polyphenol contents < 4000 were noted as poor.

3. Catalase (CAT) Activity test

CAT (conjugated self-oxidized triene) assay was performed by ultraviolet spectrophotometry. The CAT test measures the ability of a product to scavenge free radicals and evaluates the ability of the product to block oxidative free radical reactions. In this test, 2' -azo-2-aminopropane dihydrochloride (AAPH) was used to generate Reactive Oxygen Species (ROS), tung oil was used as an oxidizable substrate. The external reference used Trolox (6-hydroxy-2, 5,7, 8-tetramethyl red-2-carboxylic acid) and CAT results were expressed as Trolox equivalents per unit weight of sample. Example test results are shown in table 1.CAT value reflects the free radical scavenging ability.

Evaluation criteria for CAT value (mu mole trolox/kg): the CAT value is more than or equal to 10000 and is marked as excellent; the CAT value of 4000 is less than 10000; CAT values < 4000 were noted as poor.

4. Gallic acid content determination

Gallic acid has strong free radical scavenging ability, and is tested by high performance liquid chromatography, and the test results of example 1 and example 2 are shown in Table 2.

5. Polychlorinated biphenyls test

Referring to GB 5009.190-2014 (second method), the example test results are shown in Table 3.

6. Gandiol residual quantity test

The results of the example tests are shown in Table 4, using the gas chromatography-mass spectrometry, with reference to SN/T4505-2016.

7. Pesticide residue amount test

Referring to GB 23200.8-2016, the results of the example tests are shown in Table 5.

TABLE 1

TABLE 2

Sample number	Gallic acid content (mg/kg)
		Examples 1 to 2	380-500

TABLE 3 Table 3

TABLE 4 Table 4

Detecting items	Unit (B)	Method detection limit	Detection result
				Diethylene glycol	mg/kg	6.0	Not detected

TABLE 5

Sequence number	Detecting items	Unit (B)	Detection result	Method detection limit
					1	Alpha-hexakis	mg/kg	＜1	1
2	Beta-hexakis	mg/kg	＜1	1
					3	delta-LiuLiuLiuLiuLiuLiu	mg/kg	＜1	1
4	Gamma-hexakis	mg/kg	＜1	1
					5	o, p' -dribbling	mg/kg	＜1	1
6	p, p' -drop	mg/kg	＜1	1
					7	p, p' -Di Ji	mg/kg	＜1	1
8	p, p' -Di Ji Yi	mg/kg	＜1	1

The hybrid flower extract prepared by the technical scheme has very high total polyphenol content, capability of scavenging free radicals and excellent stability. When the polymer containing hydroxyl and ether bonds is polyglycerin-4 oleate, the total polyphenol content in the hybrid flower extract is 2-3 times that of the polyglycerin-3 diisostearate, and the free radical removing capacity is 1.4-2 times that of the polyglycerin-3 diisostearate when the polymer is 3-11% of the total weight of the raw materials; in addition, the total polyphenol content is 90-220 times that of the polyglycerol-4 oleate, and the free radical scavenging capacity is 120-460 times that of the polyglycerol-4 oleate.

Claims

1. The hybridized flower extract is characterized by comprising the following raw materials in percentage by weight: 3-11% of polymer containing hydroxyl and ether bond, 9-25% of hybrid flower, and the balance of mixed vegetable oil to 100%; the hybrid flower is black rose;

the polymer containing hydroxyl and ether bond is polyglycerol-4 oleate;

the mixed vegetable oil is jojoba oil and blackcurrant oil; the weight ratio of the jojoba oil to the blackcurrant oil is 8:1-1:8.

2. a method for preparing a hybrid flower extract according to claim 1, characterized by the steps of:

(1) Drying the hybridized flower;

(2) Grinding the hybridized flowers treated in the step (1) at the temperature of minus 60 to minus 100 ℃;

(3) Uniformly mixing the hybridized flower powder obtained by grinding in the step (2), mixed vegetable oil and a polymer containing hydroxyl and ether bonds, and then treating;

3. The method of producing a hybrid flower extract according to claim 2, wherein the water content of the hybrid flower in step (1) is 5% -20%.

4. The method of producing a hybrid flower extract according to claim 3, wherein the hybrid flower powder obtained by grinding in the step (2), the mixed vegetable oil and the polymer containing hydroxyl groups and ether bonds are uniformly mixed and subjected to microwave and ultrasonic treatment.